Triethylamine → HCID 20459476, 화합물

HRID 544129

반응식

HRID 544129 반응식
[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[NH:8][CH2:9][CH2:10][NH2:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[C:25]1([CH:31](Cl)[CH3:32])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(#N)C>[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[NH:8][CH2:9][CH2:10][NH:11][CH:31]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH3:32])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12648(1-Chloroethyl)benzeneHCID 1103156856655-17-5

생성물 1

HCID 20459476HCID 20459476, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

11 g of N-diphenylmethyl-ethylenediamine, 10.1 g of triethylamine and 7.0 g of 1-phenylethyl chloride are dissolved, while stirring, in 85 ml of acetonitrile and heated under reflux for 30 hours. The solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution are added and the mixture is extracted thoroughly by shaking with diethyl ether. The ether extracts are combined, dried over sodium sulphate and concentrated by evaporation. N-diphenylmethyl-N'-(1-phenylethyl)-ethylenediamine is obtained in the form of a yellow oil which can be purified chromatographically over silica gel with methanol/ethyl acetate (1:1) as the eluant and, for characterisation, can be converted into the dihydrochloride, having a melting point of 160° C., as described in Example 4.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 30 hours
  3. concentrationThe solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution
  4. additionare added
  5. extractionthe mixture is extracted thoroughly
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-4d3a78a70eaf4f2a8d12b6bc40eedb27
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04448776

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